A solvent-free approach is described for the regioselective synthesis of acylals (1,1-diacetates) in shorter reaction times and higher yields, compared to conventional methodology using solvents. In the protection reaction of the o-hydroxybenzaldehyde the formation of acetyl compounds and anhydro-dimers was observed. The deprotection reaction involves microwave (MW) exposure of diluted reactants in the presence of solid sulphated zirconia (SZ) catalyst that can be easily recovered and reused. The sulphated zirconia was recycled several times without any loss of activity.